SOFT 2004 Meeting Abstracts - Society of Forensic Toxicologists

M5
METHOD VALIDATION AND DETERMINATION OF MDMAAND MDA IN HAIR
Hee-Sun Chung l *, Eun-Young Hanl, Won-Kyung Yang l , Jae-Sin Lee l , Yong-Hoon Park I, Eun-Mi Kiml,
Mi-Ae Lim l and Youngchan Y002 : lNational Institute of Scientific Investigation, Seoul; 2Korea, School of
Pharmacy, Chungbuk Nat. University, Chungbuk, Korea
Recently, MDMA and MDA have been used as a recreational drug among young people in Korea. MDMA
is a substitute for methamphetamine (MA), and has recently received much attention from media and law
enforcement as a novel and popular psychoactive agent. As a result of the recent interest in designer drug,
the abuse of MDMA and MDA has increased and there were cases in which both MA and MDMA were
detected in hair samples. Therefore it was necessary for us to establish the detection method ofMDMA and
MDA in hair samples. The method validation and uncertainty measurement were also studied and
described. The prevalence of MDMA was surveyed in hair specimens submitted for drug testing by this
method.
MDMA, MDA, MDMA-ds, and MDA-ds were purchased from Radian International LLC (Austin, TX,
USA). Hair samples were collected from 791 subjects who were suspected MDMA and MDA users. After
washing, the hair was cut into small pieces of less than 1 mm and incubated. SPME extraction was applied
and extracts were derivatized by trifluoroacetic anhydride (TF A). Gas chromatograph-mass spectrometry
(GCIMS) analysis was performed under selective ion monitoring (SIM) conditions for the identification
and quantitation ofMDMA and MDA.
Limit of detection (LOD) and limit of quantitation (LOQ) of MDA and MDMA were 0.125 ng/mg,
0.25ng/mg respectively. The linear calibration curve ranged from 0.25 to 10 ng/mg with the coefficient
determination of R2 >0.99 . Within- and between run precisions were measured in three concentrations
(low 0.8 ng/mg, med 4 ng/mg, high 8 ng/mg). The specificity in blank hair and dyed artificial hair was
studied.. The high concentration of ephedrine, norephedrine, pseudoephedrine, nicotine, caffeine,
methoxyphenamine, phenterminein in low QC hair samples (0.8ng/mg) didn't show any interference in this
method. To value the confidence of the method, uncertainty was performed at the cut-off level 5 ng/mg
hair samples. The measurement in uncertainty of MDMA was ±0.22 -0.30 (95% confidence interval, k=2).
Among 791 hair samples studied, 44 hair samples were positive for MDMA or MDA (5.6 %). The
concentration of MDA was low in the hairs where both MDMA and MDA were detected indicating MDA
was the metabolite of MDMA, while in 4 specimens the level of MDA was very high with no MDMA
indicating MDA was administered. However in urine samples from same 44 subjects showed 35 were
negative for MDMA or MDA, while 9 were positive for MDMA. The hair analysis ofMDMA showed that
a hair sample is a good specimen for the confirmation of long abuse of MDMA and MDA in comparison
with urine.
Keywords: MDMA, Hair Analysis, Method Validation
Page 288